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4-Methylmorpholine → (1S)-[1-Hydroxymethyl-3-(tritylcarbamoyl)propyl]carbamic Acid Benzyl Ester

HRID 1057748
ノート
印刷プレビュー

反応式

HRID 1057748 の反応式
CN1CCOCC1.ClC(OCC)=O.[NH:14]([C:43]([O:45][CH2:46][C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1)=[O:44])[C@H:15]([C:40](O)=[O:41])[CH2:16][CH2:17][C:18](=[O:39])[NH:19][C:20]([C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[BH4-].[Na+]>C1COCC1.O>[CH2:46]([O:45][C:43](=[O:44])[NH:14][C@H:15]([CH2:40][OH:41])[CH2:16][CH2:17][C:18](=[O:39])[NH:19][C:20]([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:33]1[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1)[C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 79724-MethylmorpholineHCID 10928Ethyl chloroformateHCID 4311764Sodium borohydrideHCID 10962399Z-Gln(Trt)-OH

生成物 1

HCID 10505827(1S)-[1-Hydroxymethyl-3-(tritylcarbamoyl)propyl]carbamic Acid Benzyl Ester

試薬・触媒・溶媒 2

HCID 962Water
溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
23 °C

実験手順

4-Methylmorpholine (1.89 mL, 17.2 mmol, 1 equiv) and ethyl chloroformate (1.65 mL, 17.3 mmol, 1 equiv) were added to a mixture of commercially available Cbz-Gln(Trt)-OH (9.00 g, 17.2 mmol, 1 equiv) in THF (23 mL) at −10° C. After stirring 20 min, the reaction mixture was filtered and the filtrate was added dropwise to a suspension of NaBH4 (1.47 g, 38.9 mmol, 2.25 equiv) in H2O (10 mL) at 0° C. The resulting mixture was allowed to warm to 23° C. and stirred for 5 h. It was then cooled again to 0° C., quenched by the careful addition of 1 N HCl (30 mL) and then partitioned between MTBE (500 mL) and brine (2×100 mL). The organic phase was dried over Na2SO4 and evaporated to provide the title intermediate which was used without further purification.

後処理

  1. filtrationthe reaction mixture was filtered
  2. stirringstirred for 5 h
  3. temperatureIt was then cooled again to 0° C.
  4. customquenched by the careful addition of 1 N HCl (30 mL)
  5. custompartitioned between MTBE (500 mL) and brine (2×100 mL)
  6. dry with materialThe organic phase was dried over Na2SO4
  7. customevaporated

出典と根拠

ORDレコード
ord-922dbb5c2c104c169669214862f2bb92
出典データセット
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06514997B2

反応ノート

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